Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethyl isovalerate | HCID 7945 | — |
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Triisopropylsilyl trifluoromethanesulfonate | HCID 2724529 | — |
| Edukt | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Lösungsmittel | 2(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl- | HCID 81646 | — |
| Produkt | HCID 53927273 | HCID 53927273 | — |
Reaktionsschritte
Tetrahydrofuran (100 ml) and 1,3-dimethyl-3,4,5,6-tetrahydro 2 (1H)-pyrimidinone (140 ml) were mixed at −20° C. and lithium bis (trimethylsilyl) amide (1M in tetrahydrofuran, 100 ml) was added. The mixture was cooled to −70° C., ethyl isovalerate (18.75 ml) added and stirred for ½ hour at −70° C. Triisopropylsilyl trifluoromethane sulfonate was added and the mixture left to stir at −75° C. for ½ hour before warming to room temperature and stirring for 3 hours. The reaction mixture was quenched with aqueous sodium bicarbonate (8%, 150 ml) and extracted with hexane (1000 ml). The hexane extract was washed with water (4×500 ml), dried (MgSO4), filtered and concentrated in vacuo to afford a crude yellow oil containing the title compound.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US06215002B1 |
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| Quelldatensatz | uspto-grants-2001_04 |
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| ORD ID | ord-7bdf0bcac9b34bd9a369e584d6237570 |
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| Quellennotiz | uspto-grants-2001_04 |
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